Furfuryl Alcohol → Pyroxyfur

HRID 614080

반응식

HRID 614080 반응식
[OH-].[Na+].[OH:3][CH2:4][C:5]1[O:6][CH:7]=[CH:8][CH:9]=1.[Cl:10][C:11]1[CH:16]=[C:15]([C:17]([Cl:20])([Cl:19])[Cl:18])[CH:14]=[C:13](Cl)[N:12]=1>O>[Cl:10][C:11]1[CH:16]=[C:15]([C:17]([Cl:18])([Cl:19])[Cl:20])[CH:14]=[C:13]([O:3][CH2:4][C:5]2[O:6][CH:7]=[CH:8][CH:9]=2)[N:12]=1

참가 물질

5

반응물 3

HCID 7361Furfuryl AlcoholHCID 14798Sodium HydroxideHCID 897822,6-Dichloro-4-(trichloromethyl)pyridine

생성물 1

HCID 129813Pyroxyfur수율 87%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
50 °C

실험 절차

To 24 grams (0.6 mole) of sodium hydroxide dissolved in 120 mls of water, was added 300 mls of 2-(hydroxymethyl)furan and the solution warmed to 50° C. In this mixture was added incremently over a 20 minute period, 106.15 grams (0.4 mole) of 2,6-dichloro-4-(trichloromethyl)pyridine. The mixture was heated to ~80° C. for ~3.5 hours and thereafter diluted with water and extracted with hexane. The extract was washed with water and the hexane evaporated off leaving ~114 grams (~87 percent of theoretical) of the desired 2-chloro-6-(2-furanylmethoxy)-4-(trichloromethyl)pyridine product. The product, an oil, had a refractive index of n 25/d = 1.5722 and upon analysis was found to have carbon, hydrogen and nitrogen contents of 40.41, 2.21 and 4.21 percent, respectively, as compared with the theoretical contents of 40.40, 2.16 and 4.28 percent, respectively, as calculated for the above named compound.

후처리

  1. additionIn this mixture was added incremently over a 20 minute period
  2. temperatureThe mixture was heated to ~80° C. for ~3.5 hours
  3. extractionextracted with hexane
  4. washThe extract was washed with water
  5. customthe hexane evaporated off

출처 및 근거

ORD 기록
ord-465154c22d344e468baac5ba686cee15
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04143144

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